HCID 19828478, 화합물 → HCID 19828471, 화합물

HRID 1494526노트

반응식

HRID 1494526 반응식
CC1(C)[O:7][CH2:6][C:5]2[C:8]([CH:13]([O:21][C:22](=[O:24])[CH3:23])[C:14]3[CH:19]=[CH:18][C:17]([Cl:20])=[CH:16][CH:15]=3)=[CH:9][N:10]=[C:11]([CH3:12])[C:4]=2[O:3]1>C(O)(C(F)(F)F)=O.O>[CH3:12][C:11]1[C:4]([OH:3])=[C:5]([CH2:6][OH:7])[C:8]([CH:13]([O:21][C:22](=[O:24])[CH3:23])[C:14]2[CH:19]=[CH:18][C:17]([Cl:20])=[CH:16][CH:15]=2)=[CH:9][N:10]=1

참가 물질

3

반응물 1

HCID 19828478HCID 19828478, 화합물

생성물 1

HCID 19828471HCID 19828471, 화합물

시약·촉매·용매 1

HCID 22392675Trifluoroacetic acid water용매

실험 절차

0.24 g (0.66 mmoles) of (+)-2,2,8-trimethyl-5-(4-chloro-α-acetoxybenzyl)-pyrido-[4,3-e]-1,3-dioxane are poured into a 10 ml round bottomed flask and dissolved in 3.3 ml of TFA/H2O (10:1). The reaction is allowed to stir at room temperature for 1.5 hours, the solvent is then removed by rotary evaporation. 1 ml of methanolic ammonia is added to the crude product (the excess of TFA being neutralized), then evaporated to dryness under high vacuum. The crude product was shown to contain 90% of the desired diol-acetate by HPLC along with 4.4% of unreacted starting material.

후처리

  1. customthe solvent is then removed by rotary evaporation
  2. addition1 ml of methanolic ammonia is added to the crude product (the excess of TFA being
  3. customthen evaporated to dryness under high vacuum

출처 및 근거

ORD 기록
ord-8c32e222ef7946a19bc7c28c1fcc9760
출처 데이터셋
uspto-grants-1991_06
특허 번호
US05026855

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